Ethanol → HCID 178517575, Verbindung

HRID 2278858Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2278858
[CH:1]1([C:6](=O)[C:7]([O:9]CC)=O)[CH2:5][CH2:4][CH2:3][CH2:2]1.[F:13][C:14]1[CH:33]=[CH:32][CH:31]=[CH:30][C:15]=1[CH2:16][N:17]1[C:21]2=[N:22][CH:23]=N[CH:25]=[C:20]2[C:19]([C:26](=[NH:29])[NH:27][NH2:28])=[N:18]1.[CH2:34](O)C>>[CH:1]1([C:6]2[N:28]=[N:27][C:26]([C:19]3[C:20]4[C:21](=[N:22][CH:23]=[CH:34][CH:25]=4)[N:17]([CH2:16][C:15]4[CH:30]=[CH:31][CH:32]=[CH:33][C:14]=4[F:13])[N:18]=3)=[N:29][C:7]=2[OH:9])[CH2:2][CH2:3][CH2:4][CH2:5]1

Komponenten

4

Edukt 3

HCID 702Ethanol2×HCID 10953950Ethyl 2-cyclopentyl-2-oxoacetateHCID 178512736HCID 178512736, Verbindung

Produkt 1

HCID 178517575HCID 178517575, Verbindung

Versuchsvorschrift

1.197 g (7.035 mmol) of ethyl cyclopentyl(oxo)acetate in 15 ml of ethanol were initially introduced and heated to reflux. Then, 2.000 g (7.035 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidohydrazide suspended in 20 ml of ethanol were added and the mixture was heated under reflux overnight. After cooling, the mixture was concentrated and the residue was purified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% TFA, ratio 45:55). This gave 749 mg of the target compound (26% of theory).

Aufarbeitung

  1. temperatureheated to reflux
  2. additionwere added
  3. temperaturethe mixture was heated
  4. temperatureunder reflux overnight
  5. temperatureAfter cooling
  6. concentrationthe mixture was concentrated
  7. customthe residue was purified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% TFA, ratio 45:55)

Quellen und Nachweise

ORD-Eintrag
ord-3c2ebb481f5447a69ec8464f365e33b3
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09133191B2

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